CN104927865A - Halophosphate blue phosphor powder for white light LED and preparation method of halophosphate blue phosphor powder - Google Patents

Halophosphate blue phosphor powder for white light LED and preparation method of halophosphate blue phosphor powder Download PDF

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Publication number
CN104927865A
CN104927865A CN201510298979.XA CN201510298979A CN104927865A CN 104927865 A CN104927865 A CN 104927865A CN 201510298979 A CN201510298979 A CN 201510298979A CN 104927865 A CN104927865 A CN 104927865A
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China
Prior art keywords
phosphor powder
blue
blue phosphor
fluorescent powder
preparation
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CN201510298979.XA
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Chinese (zh)
Inventor
邓德刚
戴剑
黄君
徐时清
王焕平
华有杰
黄立辉
李晨霞
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China Jiliang University
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China Jiliang University
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Abstract

The invention discloses a halophosphate blue phosphor powder for a white light LED and a preparation method of the halophosphate blue phosphor powder. The chemical formula of the phosphor powder is Na2Ba[6-x]Gd2(PO4)6Cl2:xEu<2+>, wherein the x is equal to 0.001-0.1. The preparation method comprises the following steps: weighing corresponding raw materials of sodium chloride, barium carbonate, gadolinium oxide, ammonium dihydrogen phosphate and europium oxide according to the stoichiometric ratio of the chemical formula, then grinding and uniformly mixing the raw materials to obtain a mixture, filling the mixture into a crucible, sintering in a high temperature furnace under the condition of reducing atmosphere at 1150-1250 DEG C for 3-7 hours, and cooling to the room temperature to obtain the halophosphate blue phosphor powder. The obtained blue phosphor powder emits blue lights under the excitation of ultraviolet and a violet ray chip, and the emitting peak value is positioned around 480 nm. The phosphor powder is good in dispersivity, uniform in granularity, good in chemical stability and high in luminous efficiency, the excitation band of the phosphor powder covers the ultraviolet and the violet ray area, and the blue phosphor powder is suitable for ultraviolet LEDs.

Description

A kind of white light LEDs halogen-phosphate blue fluorescent powder and preparation method thereof
Technical field
The present invention relates to rare earth luminescent material technical field, especially relate to a kind of white light LEDs halogen-phosphate blue fluorescent powder and manufacture method thereof.
Background technology
White light LEDs is a kind of solid-state semiconductor device converting electrical energy into white light, also known as semiconductor lighting, there is the plurality of advantages such as efficiency is high, volume is little, the life-span is long, safety, low voltage, energy-saving and environmental protection, being regarded as forth generation lighting source after incandescent light, luminescent lamp, high-voltage gas discharging light by people, is the main product in following illumination market.
There is various white light LEDs preparation method at present, wherein blue-light LED chip and yellow fluorescent material combine, blue-light LED chip and red and look fluorescent material combines, purple LED chip and fluorescent material with three basic colour combine these three kinds of methods low with price, prepare the main method simply becoming and prepare white light LEDs.It is that to study also be the most ripe method the earliest that blue-light LED chip and yellow fluorescent material combine, and the white light LEDs luminous efficiency of preparation is considerably beyond incandescent light, but colour rendering index is low, and colour temperature is high, can not use as interior lighting.In order to improve the color developing of white light LEDs, various countries scientist have developed blue-light LED chip and red, look fluorescent material combines and purple LED chip and red, blue fluorescent material with three basic colour combines other two kinds of methods realizing white light LEDs.
The emission wavelength of current InGaN chip moves near ultraviolet region, can provide higher excitation energy for fluorescent material, improves the light intensity of white light LEDs further.Because UV-light is invisible, the color of burst of ultraviolel white light LEDs can only be determined by fluorescent material, therefore colour stable, colour rendering index is high, uses near ultraviolet InGaN chip and blue, yellow fluorescent material or becomes the emphasis of current white light LEDs industry development with the scheme that three primary colors fluorescent powder combines to realize white light.Blue colour fluorescent powder is indispensable composition in the program.
LED blue colour fluorescent powder is mainly divided into several large system: sulphide fluorescent material, aluminate fluorescent powder, silicate fluorescent powder, phosphate phosphor and silica-based nitrogen (oxygen) compound fluorescent material.Sulfide blue colour fluorescent powder is as CaLaGa 3s 6o:Eu 2+.Aluminate blue fluorescent powder is as BaMgAl 10o 17: Eu 2+.Silicate blue fluorescent powder is as MSiO 4: Eu 2+(M=Ca, Sr, Ba), Y 2siO 5: Ce 3+, SrAl 2si 2o 8: Eu 2+, M 3mgSi 2o 8: Eu 2+(M=Ba, Sr) etc.Phosphate phosphor is as LiSrPO 4: Eu 2+, KSrPO 4: Eu 2+and SrMg 2(PO 4) 2: Eu 2+deng.Silica-based nitrogen (oxygen) compound blue colour fluorescent powder is as BaSi 2o 2n 2: Eu 2+, Ca 2si 5n 8: Ce 3+and Ba 2si 5n 8: Ce 3+deng.
Summary of the invention
The object of this invention is to provide a kind of white light LEDs halogen-phosphate blue fluorescent powder and preparation method thereof.
For achieving the above object, the technical solution used in the present invention is: its white light LEDs halogen-phosphate blue fluorescent powder has following chemical representation: Na 2ba 6-xgd 2(PO 4) 6cl 2: xEu 2+, in formula, x is 0.001 ~ 0.10.
The preparation method of halogen-phosphate blue fluorescent powder of the present invention comprises the steps:
By chemical formula Na 2ba 6-xgd 2(PO 4) 6cl 2: xEu 2+stoichiometric ratio take corresponding raw material, described raw material is respectively sodium-chlor, barium carbonate, gadolinium sesquioxide, primary ammonium phosphate and europium sesquioxide, and wherein x is 0.001 ~ 0.1; Be ground and obtain mixture; This mixture is loaded crucible, and in High Temperature Furnaces Heating Apparatus, sinter 3 ~ 7 hours under reducing atmosphere and 1150 ~ 1250 DEG C of conditions, rear cool to room temperature obtains described halogen-phosphate blue fluorescent powder.
Further, reducing atmosphere of the present invention is nitrogen and hydrogen mixture or CO atmosphere.
Compared with prior art, the invention has the beneficial effects as follows:
(1) fluorescent material of the present invention is substrate material with halogen-phosphate, has chemical stability and good thermal stability, and raw material is inexpensive, be easy to get, the advantages such as sintering temperature is low.Compare sulfide blue colour fluorescent powder, Heat stability is good of the present invention.Compare aluminate blue fluorescent powder, preparation temperature of the present invention is lower than aluminate, and particle is thinner than aluminate, and luminosity is high and luminous efficiency is high.Compare silicate blue fluorescent powder, grain graininess of the present invention is even, and sintering temperature is low.Compare silica-based nitrogen (oxygen) compound blue colour fluorescent powder, sintering temperature of the present invention is low, and synthesis technique is simple and raw material is cheap and easy to get.
(2) the present invention compares other phosphate blue fluorescent powders (as LiSrPO 4: Eu 2+, KSrPO 4: Eu 2+), avoid with deliquescent alkaline carbonate in high, the exposure air of decomposition temperature.
Accompanying drawing explanation
Fig. 1 is the fluorescent powder exciting light spectrogram (supervisory wavelength 480 nanometer) of embodiment 1 provided by the invention preparation;
Fig. 2 is the fluorescent powder utilizing emitted light spectrogram (excitation wavelength 470 nanometer) of embodiment 1 provided by the invention preparation;
Fig. 3 is fluorescent powder XRD figure spectrum and the Na of embodiment 1 provided by the invention preparation 2ba 6eu 2(PO 4) 6cl 2(JCPDF29-1172) standard diagram;
Fig. 4 is that the fluorescent powder TEM of embodiment 1 provided by the invention preparation schemes.
Embodiment
Below in conjunction with drawings and Examples, this patent is further explained.
Embodiment 1:
A kind of white light LEDs halogen-phosphate blue fluorescent powder, according to Na 2ba 5.995gd 2(PO 4) 6cl 2: 0.005Eu 2+take NaCl, BaCO 3, Gd 2o 3, NH 3h 2pO 4and Eu 2o 3, the mol ratio between them is 2:5.995:1:6:0.0025, and after abundant ground and mixed is even, place in corundum crucible, then put into High Temperature Furnaces Heating Apparatus 1150 DEG C of roastings 3 hours under CO atmosphere, rear cool to room temperature, obtains halogen-phosphate blue fluorescent powder.
As can be seen from Figure 1, the fluorescent material excitation spectrum of the present embodiment is a wide range, covers ultraviolet, purple light and blue light region, and excitation peak is positioned near 370nm, illustrates that the fluorescent material of the present embodiment effectively can be excited by blue light or purple light chip.When the excitation wavelength of emmission spectrum is 370nm, as can be seen from Figure 2, the broadband blue light being emitted as divalent europium of the fluorescent material of the present embodiment is launched, and emission peak is positioned near 470nm, illustrates that the fluorescent material of the present embodiment is applicable to doing ultraviolet, purple light or blue-light excited blue colour fluorescent powder.As can be seen from Figure 3, the powder X-ray diffraction peak of the present embodiment and Na 2ba 6eu 2(PO 4) 6cl 2(JCPDF29-1172) standard diagram coincide better, illustrates that the powder thing of the present embodiment is compared pure.As can be seen from Figure 4, the diameter of particle of the present embodiment, at 10 microns, has good dispersiveness.
Embodiment 2:
A kind of white light LEDs halogen-phosphate blue fluorescent powder, according to Na 2ba 5.999gd 2(PO 4) 6cl 2: 0.001Eu 2+, take NaCl, BaCO 3, Gd 2o 3, NH 3h 2pO 4and Eu 2o 3, the mol ratio between them is 2:5.999:1:6:0.0005, and after abundant ground and mixed is even, place in corundum crucible, then put into High Temperature Furnaces Heating Apparatus 1250 DEG C of roastings 7 hours under CO atmosphere, rear cool to room temperature, obtains halogen-phosphate blue fluorescent powder.
The fluorescent material excitation spectrum of the present embodiment is a wide range, covers ultraviolet, purple light and blue light region, and excitation peak is positioned near 370nm, illustrates that the fluorescent material of the present embodiment effectively can be excited by blue light or purple light chip.When the excitation wavelength of emmission spectrum is 370nm, the broadband blue light being emitted as divalent europium of the fluorescent material of this enforcement is launched, and emission peak is positioned near 475nm, illustrates that the fluorescent material of the present embodiment is applicable to doing ultraviolet, purple light or blue-light excited blue colour fluorescent powder.The diameter of particle of the present embodiment, at 15 microns, has good dispersiveness.
Embodiment 3:
A kind of white light LEDs halogen-phosphate blue fluorescent powder, according to Na 2ba 5.99gd 2(PO 4) 6cl 2: 0.01Eu 2+take NaCl, BaCO 3, Gd 2o 3, NH 3h 2pO 4and Eu 2o 3, the mol ratio between them is 2:5.99:1:6:0.005, and after abundant ground and mixed is even, place in corundum crucible, then put into High Temperature Furnaces Heating Apparatus 1150 DEG C of roastings 7 hours under CO atmosphere, rear cool to room temperature, obtains halogen-phosphate blue fluorescent powder.
The fluorescent material excitation spectrum of the present embodiment is a wide range, covers ultraviolet, purple light and blue light region, and excitation peak is positioned near 370nm, illustrates that the fluorescent material of the present embodiment effectively can be excited by blue light or purple light chip.When the excitation wavelength of emmission spectrum is 370nm, the broadband blue light being emitted as divalent europium of the fluorescent material of this enforcement is launched, and emission peak is positioned near 478nm, illustrates that the fluorescent material of the present embodiment is applicable to doing ultraviolet, purple light or blue-light excited blue colour fluorescent powder.The diameter of particle of the present embodiment, at 10 microns, has good dispersiveness.
Embodiment 4:
A kind of white light LEDs halogen-phosphate blue fluorescent powder, according to Na 2ba 5.95gd 2(PO 4) 6cl 2: 0.05Eu 2+take NaCl, BaCO 3, Gd 2o 3, NH 3h 2pO 4and Eu 2o 3, the mol ratio between them is 2:5.95:1:6:0.025, after abundant ground and mixed is even, places in corundum crucible, then puts into High Temperature Furnaces Heating Apparatus in 5%H 2+ 95%N 21200 DEG C of roastings 2 hours under the nitrogen and hydrogen mixture atmosphere of (volume ratio), rear cool to room temperature, obtains halogen-phosphate blue fluorescent powder.
The fluorescent material excitation spectrum of the present embodiment is a wide range, covers ultraviolet, purple light and blue light region, and excitation peak is positioned near 370nm, illustrates that the fluorescent material of the present embodiment effectively can be excited by blue light or purple light chip.When the excitation wavelength of emmission spectrum is 370nm, the broadband blue light being emitted as divalent europium of the fluorescent material of this enforcement is launched, and emission peak is positioned near 480nm, illustrates that the fluorescent material of the present embodiment is applicable to doing ultraviolet, purple light or blue-light excited blue colour fluorescent powder.The diameter of particle of the present embodiment, at 12 microns, has good dispersiveness.
Embodiment 5:
A kind of white light LEDs halogen-phosphate blue fluorescent powder, according to Na 2ba 5.9gd 2(PO 4) 6cl 2: 0.1Eu 2+take NaCl, BaCO 3, Gd 2o 3, NH 3h 2pO 4and Eu 2o 3, the mol ratio between them is 2:5.9:1:6:0.05, after abundant ground and mixed is even, places in corundum crucible, then puts into High Temperature Furnaces Heating Apparatus in 5%H 2+ 95%N 21250 DEG C of roastings 3 hours under the nitrogen and hydrogen mixture atmosphere of (volume ratio), rear cool to room temperature, obtains halogen-phosphate blue fluorescent powder.
The fluorescent material excitation spectrum of the present embodiment is a wide range, covers ultraviolet, purple light and blue light region, and excitation peak is positioned near 370nm, illustrates that the fluorescent material of the present embodiment effectively can be excited by blue light or purple light chip.When the excitation wavelength of emmission spectrum is 370nm, the broadband blue light being emitted as divalent europium of the fluorescent material of this enforcement is launched, and emission peak is positioned near 480nm, illustrates that the fluorescent material of the present embodiment is applicable to doing ultraviolet, purple light or blue-light excited blue colour fluorescent powder.The diameter of particle of the present embodiment, at 15 microns, has good dispersiveness.
Above-described embodiment is used for explaining and the present invention is described, instead of limits the invention, and in the protection domain of spirit of the present invention and claim, any amendment make the present invention and change, all fall into protection scope of the present invention.

Claims (3)

1. a white light LEDs halogen-phosphate blue fluorescent powder, is characterized in that, this fluorescent material has following chemical representation: Na 2ba 6-xgd 2(PO 4) 6cl 2: xEu 2+, wherein, x is 0.001 ~ 0.1.
2. a preparation method for halogen-phosphate blue fluorescent powder according to claim 1, is characterized in that comprising the steps:
By chemical formula Na 2ba 6-xgd 2(PO 4) 6cl 2: xEu 2+stoichiometric ratio take corresponding raw material, described raw material is respectively sodium-chlor, barium carbonate, gadolinium sesquioxide, primary ammonium phosphate and europium sesquioxide, and wherein x is 0.001 ~ 0.1; Be ground and obtain mixture; This mixture is loaded crucible, and in High Temperature Furnaces Heating Apparatus, sinter 3 ~ 7 hours under reducing atmosphere and 1150 ~ 1250 DEG C of conditions, rear cool to room temperature obtains described halogen-phosphate blue fluorescent powder.
3. the preparation method of halogen-phosphate blue fluorescent powder as claimed in claim 2, is characterized in that: described reducing atmosphere is nitrogen and hydrogen mixture or CO atmosphere.
CN201510298979.XA 2015-06-03 2015-06-03 Halophosphate blue phosphor powder for white light LED and preparation method of halophosphate blue phosphor powder Pending CN104927865A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107841308A (en) * 2016-09-20 2018-03-27 南京工业大学 A kind of purple light excited halogen-phosphate blue-green fluorescent powder and preparation method thereof
CN109777422A (en) * 2019-03-18 2019-05-21 旭宇光电（深圳）股份有限公司 Suitable for purple light excited blue colour fluorescent powder and preparation method thereof and light emitting device
CN110157432A (en) * 2019-05-14 2019-08-23 南京科津新材料研究院有限公司 A kind of white fluorescent powder and preparation method thereof, white light LED part and preparation method thereof
CN110791291A (en) * 2019-09-29 2020-02-14 贺州学院 Synthesis method of phosphosilicate white light emitting fluorescent powder
CN110894425A (en) * 2019-11-27 2020-03-20 南京邮电大学 Rare earth and metal ion doped phosphor with light temperature sensing and multiband light emission functions and preparation method thereof
CN111647406A (en) * 2020-06-15 2020-09-11 南京工业大学 Fluorescent powder and preparation method thereof
CN116575107A (en) * 2022-11-01 2023-08-11 广州珠江光电新材料有限公司 Preparation method of blue fluorescent powder, product and application thereof

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107841308A (en) * 2016-09-20 2018-03-27 南京工业大学 A kind of purple light excited halogen-phosphate blue-green fluorescent powder and preparation method thereof
CN109777422A (en) * 2019-03-18 2019-05-21 旭宇光电（深圳）股份有限公司 Suitable for purple light excited blue colour fluorescent powder and preparation method thereof and light emitting device
CN109777422B (en) * 2019-03-18 2021-06-25 旭宇光电（深圳）股份有限公司 Blue fluorescent powder suitable for purple light excitation, preparation method thereof and light-emitting device
CN110157432A (en) * 2019-05-14 2019-08-23 南京科津新材料研究院有限公司 A kind of white fluorescent powder and preparation method thereof, white light LED part and preparation method thereof
CN110791291A (en) * 2019-09-29 2020-02-14 贺州学院 Synthesis method of phosphosilicate white light emitting fluorescent powder
CN110894425A (en) * 2019-11-27 2020-03-20 南京邮电大学 Rare earth and metal ion doped phosphor with light temperature sensing and multiband light emission functions and preparation method thereof
CN111647406A (en) * 2020-06-15 2020-09-11 南京工业大学 Fluorescent powder and preparation method thereof
CN116575107A (en) * 2022-11-01 2023-08-11 广州珠江光电新材料有限公司 Preparation method of blue fluorescent powder, product and application thereof

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Application publication date: 20150923